Sulfur color and process of making same.



colonfoi'ming propertiesffor eX'aInple',"by

UNITED STATES rATEN-T OFFICE.

EMILE THEODORE BUND SM AN OFPOINT L'OMA, CALIFORNIA, ASSIG NOR 'IO.IHE POINT LOMA CHEMICAL COMPANY, OF- POINT LOMA CALIFORNIA, A CORPORATION OF SOUTH DA- KOTA.

SULFUIB AND PROCESS OF MAKING SAME.

Application filed. October-7, 1905. Serial Nb. 281,762.

To all tvhom it may concern: I

Be it known that I, EMILE THEODORE BUnnsMAN, a citizen of the United States, residing at Point Lorna, San Diego county, in the State of California, have invented a new and useful Improvement in Coloring- Matters and Processes of Making the Same, of which the follovving' is a specification.

Thavediscovered that the members of the group of chemicalsknown as the sugars may beused in combination with other chemicals to produce coloring'rnatt-ers'.

The sugars will, Whe'n-sulfurized by any of the sulfuring agents-of the arts, in-oombination with. such other chemicals as can themselvesbesulfurized to form colors, produce, valuablegandnew coloring matters.

These coloring matters possess properties which are usually markedly different from' those possessed by coloring matters produced by sulfuring the other color-forming chen1-- ters are produced. The sugars may there;

fore be said to play thepart of co-bases. These ne u co-bases may be sulfured inconnection with an unlimited number of other color-forming.chemicals, and in -each instance anew coloring matter obtained; they seem, therefore, to be unlversal 1n their, ap-

'plication, and to be properly designated as f universal'co-bases. They seem to occupy aunique position in the manufacture of coloring matters, no other color base having as yet been found to have similar universal applicability. New and valuable coloring matters may furthermore be produced by sulfuring the sugars in connection with other chemicals'wliich, while belonging to the same groups as those already described and having many analogies to suchchemicals, do not in themselves possess similar sulfuring the sugars in combination with aromatic; chemicals whichwill' not, with sulfuring agents alone, produce coloring matters' The sugars, therefore, seem to give color-forming properties to such noncoloz foi i ning chemicals, I have caused e};-

Specification of Letters Patent.

. Patented Jan. 12, 1909.

periments to be made with a number of non color forming, aromatic chem1cals, and, in

each instance, a new coloring matter has: been produced. The sugars occupy a unique and technically, are given by the use of grape sugar, although the other sugars, as glucose or cane sugar, g ve excellent results.

trate the manner in which coloring matters may belproduced from the-sugars in combination with other chemicals.

Example I. A sugar used us co-tasis, in

' Thefollotving examples will serve to illusconnection with a color-forming chemical-e .Weigh out into a suitable crucible: 8 parts grape sugar, 12 parts s'ulfur,'60 parts sodium sulhd crystals. Apply heat and raise the temperature to 120 C. After one hour at this temperature, dissolve in water, cool, and add 6 parts of inetamitranilin. 1 Raise the heat to drive off the Water. Then raise the temperature gradually but steadily to. 2503G O C. and heat until a dry mass is formed, which can be readily pulverized, and until a dyeing test shows that full tinctorial power has been developed. The process takes from seven to eight hours in all. The fulltinctorial power of the color is best developed .by this process, although a similar color will be produced when the 'meta nitranilin is added in the beginning. i

The substance obtained by this process is soluble in cold water, cold sodium carbonate solution, alcohol and caustic alkaline solution, and dyes unmordanted cotton 2. fast bright, yellowish brown shade in the usual alkaline salt bath, with or without the addition of sodium sulfid. The color may also be concentrated. in the usual manner by pre cipitation with hydrochloric acid, the resulting substance being insoluble in cold soluble in cold sodium sulfid solution. It dyes unmordanted' cottona fast, bright yellowish brown shade, in an alkaline salt bath With the assistance of sodium suliid. When identically the same operation is performed with v out the grape sugar, a dull greenish black alone is formed.

This example illustrates a'great number of syntheses of coloring matters that can be performed by the-use of these universal cobases in combination with other chemicals which are themselves color bases. Thus, by substituting for meta-nitranilin either metaphenylene diamin base or meta-dinitro benzene, in the above formula, browns will be formed somewhat similar to the brown obtained from meta-nitranilin. By usingparanitrophenol a darker yellow brown is obtained. Binitrochl0rbenzol yields a val uable medium brown. 1.8 dinitro-naphtha lene yields'a valuable black.

Variations of temperature will produce a variation in the shade of the product. By varying the proportions of the ingredients other variations in color can be produced.

Example 11. A sugar used to impart colorforming properties to a chemical which, under similar circumstances and conditions, is not a colorformer.Weigh out intoa suitable crucible: 8 parts grape sugar, 12 .parts sulfur, 60 parts sodium sulfid crystals. Apply heat and raise the temperature to 120 C. After one hour at this temperature dissolve in water, cool, and add 6 parts of sodium salt of sulfanilic acid. liaise. the heat to drive off the water, then raise'the heat gradually but steadily to 150-1S0 C., and heat'until a dry owder is formed, or a dyeing test of the sion shows that the colorhas been fully vformed.

The above process. gives the best result, although a similar result is obtained by add ing the sodium salt of sulfanilic acid in the beginning. The resulting substance is soluble in cold water, cold'sodium carbonate solution, alcohol, and caustic alkaline solut1on, and dyes unmordanted cotton a fast medium brown in a salt bath made alkaline .with soda, with or without the addition of sodium sulfid'. It may also be concentrated in the usual manner by precipitation with hydro'ohloricacid, in which case the result- -Lug-substance will be insoluble in cold water, cold sodium carbonate solution, alcohol, and

concentrated sulfuric acid, slowly soluble in caustic alkaline solution and readily soluble incold sodium suliid solution. It will dye unmordaiited cotton a fast medium brown in the usual alkaline salt bath, with the as-- sistance of sodium Variations of temperature will produce a shade of the product. By varying the proportions of the ingredients other variationsv in color can be'produced.

When the same operation is erformed without: the grape sugar, no color is formed.

scams This example illustrates a great number of syntheses ofcoloring matters that can be performed by the use of these universal color formers. Thus by substituting for the sodium salt of sulfanilic acid in-the above formula, either anilin salts, benzidin, or diphenylamin, chemicals which are not color formers, otherand new colors will be proiembers of the so-called group of aromatic Coloring. matters have been chemicals. produced by the sulfurmg of grape sugar in combination with a number of aromatic duced, such as dark red with anilin salts,

chemicals, both of those having color-forming properties when sulfured, and those not.

possessing color forming properties under the same treatment. The examples above referred to all involve'the use of an aromatic chemical. While the sugars in combination with. many chemicals will produce coloring matters, they-are particularly suited to form coloring matters in combination with such aromatic chemicals.

1 claim as my invention:

1.. The process of making suh'ur dyes con sisting in heating a mixture of a sugar, a color forming aromatic chemical, and a sulfuring agent.

2. The process of sisting in heating grape sugar, a color-forming aromatic chemical, and a sulfuring agent.

making sulfur dyes, con- 3. The process of making a sulfur dye, consisting in heating a mixture of sugar, metanitranilin, and a sulfuring agent, substantially as described. I

4E. The process of making a sulfur dye, consisting in heating a mixture of grape sugar, meta-nitranilin, and a sulfuring agent, substantially as described.

5. As a new article of manufacture, the coloring matter which can be made from grape sugar and meta-nitranilin, substantially as described, which is soluble in cold water, cold sodium carbonate solution, alco" hol. end caustic alkaline solution, andwhich dyes cotton in alkaline salt bath, fast brown shades. e

6. As new article of manufacture, the coloring matter which is precipitated by hydroc'hlorie acid from a solution of the coloring matter made from grape sugar and met nitranilin, substantially as described, which is insoluble in cold water, coldsodiirm carbonate solution, alcohol, and concentrated sulfusigned my name in'the presence of two subric acid, which is slowly soluble in caustic alscribing witnesses. kaline solution, which is readily soluble in cold.

sodium sulfid solution, and dyes cotton from y EMILE THEODORE BUNDSMAN 5 an alkaline salt bath with theassistance of Witnesses: j

sodium sulfid, fast brown shades. G. THUR'S'TON,

In testimony whereof, I have hereunto v DEBpR oKER. 

